Submicrometre-resolution polychromatic three-dimensional X-ray microscopy

2012 ◽  
Vol 46 (1) ◽  
pp. 153-164 ◽  
Author(s):  
B. C. Larson ◽  
L. E. Levine

The ability to study the structure, microstructure and evolution of materials with increasing spatial resolution is fundamental to achieving a full understanding of the underlying science of materials. Polychromatic three-dimensional X-ray microscopy (3DXM) is a recently developed nondestructive diffraction technique that enables crystallographic phase identification, determination of local crystal orientations, grain morphologies, grain interface types and orientations, and in favorable cases direct determination of the deviatoric elastic strain tensor with submicrometre spatial resolution in all three dimensions. With the added capability of an energy-scanning incident beam monochromator, the determination of absolute lattice parameters is enabled, allowing specification of the complete elastic strain tensor with three-dimensional spatial resolution. The methods associated with 3DXM are described and key applications of 3DXM are discussed, including studies of deformation in single-crystal and polycrystalline metals and semiconductors, indentation deformation, thermal grain growth in polycrystalline aluminium, the metal–insulator transition in nanoplatelet VO2, interface strengths in metal–matrix composites, high-pressure science, Sn whisker growth, and electromigration processes. Finally, the outlook for future developments associated with this technique is described.

2011 ◽  
Vol 681 ◽  
pp. 1-6 ◽  
Author(s):  
Denis Bouscaud ◽  
Raphaël Pesci ◽  
Sophie Berveiller ◽  
Etienne Patoor

A Kossel microdiffraction experimental set up is under development inside a Scanning Electron Microscope (SEM) in order to determine the crystallographic orientation as well as the inter- and intragranular strains and stresses. An area of about one cubic micrometer can be analysed using the microscope probe, which enables to study different kinds of elements such as a grain boundary, a crack, a microelectronic component, etc. The diffraction pattern is recorded by a high resolution Charge-Coupled Device (CCD) camera. The crystallographic orientation, the lattice parameters and the elastic strain tensor of the probed area are deduced from the pattern indexation using a homemade software. The purpose of this paper is to report some results achieved up to now to estimate the reliability of the Kossel microdiffraction technique.


2009 ◽  
Vol 19 (12) ◽  
pp. 2231-2262 ◽  
Author(s):  
JENS FREHSE ◽  
DOMINIQUE LÖBACH

For a flat Dirichlet boundary we prove that the first normal derivatives of the stresses and internal parameters are in L∞(0, T; L1+δ) and in L∞(0, T; H½-δ) up to the boundary. This deals with solutions of elastic–plastic flow problems with isotropic or kinematic hardening with von Mises yield function. We show that the elastic strain tensor ε(u) of three-dimensional plasticity with isotropic hardening is contained in the space [Formula: see text] and in L∞(0,T;H4-δ) up to the flat Dirichlet boundary. We obtain related results concerning traces of ε(u). In the case of kinematic hardening we present a simple proof of the [Formula: see text] inclusion of the elastic strain tensor.


2019 ◽  
Vol 52 (5) ◽  
pp. 1128-1143 ◽  
Author(s):  
Miguel Angel Vicente Alvarez ◽  
Javier Santisteban ◽  
Gladys Domizzi ◽  
John Okasinski ◽  
Jonathan Almer

Zirconium alloys are used in fuel cladding and structural components of nuclear power plants. Hydrogen enters the Zr matrix during plant operation and precipitates as hydride particles that degrade the mechanical properties of the alloy, limiting service life. Knowledge of the stress state within hydride precipitates is important to understand stress-induced degradation mechanisms such as delayed hydride cracking, but no direct quantification has yet been reported in the literature. Here, measurements are reported of the average elastic strain tensor within δ zirconium hydride precipitates in Zr2.5%Nb pressure tube material from CANDU power plants. Complete intensity and strain pole figures for the hydride were obtained by synchrotron X-ray diffraction experiments on specimens with hydrogen contents ranging from ∼100 wt p.p.m. hydrogen to nearly 100% δ-hydride. Zirconium hydride precipitates by a process involving a martensitic transformation, with two hydride variants possible from a single α-Zr grain. A synthetic model of the hydride crystallographic texture allowed the interpretation of the measured strain pole figures and quantification of the elastic strain tensor for both texture components. It was found that the two variants appear in nearly equal proportion but with different stress states, differing in the sign of the shear strain components (∼±3000 µ∊). This difference is possibly associated with the shear movement of Zr atoms during the phase transformation. This suggests that hydride clusters are composed of stacks of smaller hydrides in alternating hydride variants. Stresses were estimated from a set of rather uncertain hydride elastic constants. Overall, both variants showed compressive strains along the tube axial direction (∼5000 µ∊). For low hydrogen concentrations, the hydrides' stress tensor is dominated by compressive stresses of ∼300 MPa along the axial direction, probably caused by the elongated morphology of hydride clusters along this direction, and variant-dependent shear stresses of ∼±100 MPa, probably from the shear movement of the Zr atoms involved in the phase transformation.


Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.


2008 ◽  
Vol 77 (1) ◽  
Author(s):  
Hidekazu Mimura ◽  
Hirokatsu Yumoto ◽  
Satoshi Matsuyama ◽  
Soichiro Handa ◽  
Takashi Kimura ◽  
...  

1987 ◽  
Vol 26 (Part 1, No. 1) ◽  
pp. 157-161 ◽  
Author(s):  
Osamu Nittono ◽  
Yoshihiro Sadamoto ◽  
Sheng Kai Gong

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